7-Sep-21 News Some tips on 4535-90-4

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Quality Control of 2-Chloro-N-methylethanamine hydrochloride

Water (0.5 mL), intermediate 17 (0.17 g; 0.51 mmol) followed by tetrabutylammonium bromide (41 mg; 0.13 mmol) were added at room temperature to a mixture of potassium hydroxide (0.50 g; 7.63 mmol) in 2-methyltetrahydrofuran (5 mL). The reaction mixture was stirred for 10 minutes at room temperature, then stirred at 50C for 1 hour and (2- chloroethyl)-methylamine hydrochloride (CAS 4535-90-4) (0.119 g; 0.92 mmol) was added. The reaction mixture was stirred for 24 hours at 50C. The reaction mixture was cooled down to room temperature, poured into water and extracted with EtOAc. The organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The residue was purified by chromatography over silica gel (Spherical SiOH, 10muiotaeta, 60g; mobile phase: gradient from 0.5% NH4OH, 97% DCM, 3% MeOH to 0.5% NH OH, 95% DCM, 5% MeOH). The pure fractions were collected and evaporated to give 30 mg (15%) which was taken up Et20 and evaporated to give 29 mg (14%) of compound 44 , MP.: 80C (gum, Kofler).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; SAXTY, Gordon; ANGIBAUD, Patrick Rene; QUEROLLE, Olivier Alexis Georges; PONCELET, Virginie Sophie; ROUX, Bruno; MEERPOEL, Lieven; WO2013/61080; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 2-Chloro-N-methylethanamine hydrochloride

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-methylethanamine hydrochloride, its application will become more common.

Synthetic Route of 4535-90-4,Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A solution of 50 mg of 3-((2-(4-((3-(trifluoromethyl)benzyl)carbamoyl)pyridin-2-yl)-4-(piperidin-1-yl)phenyl)carbamoyl)benzoic acid 4.1e, 9.3 mg of N-methyl-N-(2-chloroethyl)amine hydrochloride, 43 muL of diisopropylethylamine, and 35 mg of HATU in 1000 muL of DMF was stirred for 1 h. The mixture was diluted with 20 mL of water, and the resulting precipitate was collected by filtration. It was dissolved in dichloromethane and the solution was washed with water and dried (Na2SO4). The solvent was evaporated to give 42 mg of product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-methylethanamine hydrochloride, its application will become more common.

Reference:
Patent; Ardelyx, Inc.; Lewis, Jason G.; Jacobs, Jeffrey W.; Reich, Nicholas; Leadbetter, Michael R.; Bell, Noah; Chang, Han-Ting; Chen, Tao; Navre, Marc; Charmot, Dominique; Carreras, Christopher; Labonte, Eric; (323 pag.)US9301951; (2016); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Extracurricular laboratory: Synthetic route of 4535-90-4

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Related Products of 4535-90-4,Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A9. (3RS,3aRS)-8-Fluoro-3-phenyl-3a,4-dihydro-3H-chromeno[4,3-c]pyrazole-2-carboxylic acid (2-chloro-ethyl)-methyl-amide; To an ice cold solution of 636 mg (1.92 mmol) (3RS,3aRS)-8-Fluoro-3-phenyl-3a,4-dihydro-3H-chromeno[4,3-c]pyrazole-2-carbonyl chloride (compound A7) in 40 ml dichloromethane are added 389 mg (3.85 mmol) triethyl amine and after 30 min a solution of 250 mg (1.92 mmol) 2-methylaminoethylchloride hydrochloride in 7 ml methanol. The mixture is stirred for 1 h at room temperature. Additional dichloromethane and a diluted aqueous solution of hydrochloric acid are added. The organic layer is dried with magnesium sulfate. The solvents are removed at reduced pressure. The crude product is purified by column chromatography (silica gel, light petroleum/ethyl acetate 2:1). 515 mg of the title compound are obtained as a yellowish solid. (m/z (MH+)=388.1).

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vennemann, Matthias; Baer, Thomas; Maier, Thomas; Lindenmaier, Andreas; Braunger, Juergen; Boehm, Markus; Zimmermann, Astrid; Gekeler, Volker; US2010/104659; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of C3H9Cl2N

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: C3H9Cl2N

A suspension of N-Methyl-2-chloroethylammonium chloride (10 gm) in POCl3 (40 ml) was refiuxed (1350C) over night. After removing excess POCl3 under vacuum product 5i was distilled out under vacuum as light yellow oil and analyzed by 1H and 31P NMR spectroscopy to be pure.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; THRESHOLD PHARMACEUTICALS, INC.; WO2007/2931; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on C3H9Cl2N

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-methylethanamine hydrochloride, its application will become more common.

Related Products of 4535-90-4,Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

(ii) The white crystal 3 (1.0 g, 7.69 mmol) and sodium thiosulfate pentahydrate (1.91 g, 7.69 mmol) were added into 100 mL flask. MilliQ water (10 mL) was then added into the flask, and the reaction mixture was stirred at 120 C for 24 h under argon atmosphere. The reaction was then cooled to room temperature and the solvent was removed under reduced pressure. Hydrochloric acid (6.0 M, 25 mL) was added into the flask and the solution was stirred at 85 C for 3 h under argon atmosphere. The solvent was then removed, and 100 mL of dichloromethane and 15 mL of ethanol were added to extract the product. Sodium chloride and sulfate salts were precipitated from the solution. The salts were then filtered and the filtrate was concentrated to give product as a white solid (0.55 g, yield: 56.1%). The B monomer was extremely hygroscopic, which was needed to be stored in a dry oven. The 1H NMR and 13C NMR spectra of B monomer were shown in Fig. S4.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-methylethanamine hydrochloride, its application will become more common.

Reference:
Article; Xu, Chao-Ran; Zhang, Ze; Pan, Cai-Yuan; Hong, Chun-Yan; Polymer; vol. 172; (2019); p. 294 – 304;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Extended knowledge of C3H9Cl2N

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 2-Chloro-N-methylethanamine hydrochloride

(a) 1-Benzyl-3-(2-chloroethyl-methyl-amino)-pyrrolidine-2,5-dione 74.8 g (0.4 mol) of N-benzylmaleimide [Arch. Pharm. 308, 489 (1975)] and 52.0 g (0.4 mol) of 2-chloroethyl-methylamine hydrochloride are initially introduced into 400 ml of dioxane and 40.4 g (0.4 mol) of triethylamine are added dropwise at 20 C. The mixture is then boiled under reflux for 5 hours. The batch is subsequently poured into 2 l of ice-water and extracted with 3 portions of 400 ml of chloroform and the extract is washed with water, dried over sodium sulphate and concentrated on a rotary evaporator. Chromatography of the residue (101.1 g) on silica gel using ethyl acetate:petroleum ether (1:2) gives 56.8 g (51% of theory) of an oil. RF value: 0.33 (silica gel, ethyl acetate/petroleum ether=1:2)

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Aktiengesellschaft; US4990517; (1991); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 4535-90-4

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Chloro-N-methylethanamine hydrochloride

Water (0.5 mL), intermediate 17 (0.17 g; 0.51 mmol) followed by tetrabutylammonium bromide (41 mg; 0.13 mmol) were added at room temperature to a mixture of potassium hydroxide (0.50 g; 7.63 mmol) in 2-methyltetrahydrofuran (5 mL). The reaction mixture was stirred for 10 minutes at room temperature, then stirred at 50C for 1 hour and (2- chloroethyl)-methylamine hydrochloride (CAS 4535-90-4) (0.119 g; 0.92 mmol) was added. The reaction mixture was stirred for 24 hours at 50C. The reaction mixture was cooled down to room temperature, poured into water and extracted with EtOAc. The organic layer was washed with brine, dried over MgS04, filtered and evaporated to dryness. The residue was purified by chromatography over silica gel (Spherical SiOH, 10muiotaeta, 60g; mobile phase: gradient from 0.5% NH4OH, 97% DCM, 3% MeOH to 0.5% NH OH, 95% DCM, 5% MeOH). The pure fractions were collected and evaporated to give 30 mg (15%) which was taken up Et20 and evaporated to give 29 mg (14%) of compound 44 , MP.: 80C (gum, Kofler).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; BERDINI, Valerio; SAXTY, Gordon; ANGIBAUD, Patrick Rene; QUEROLLE, Olivier Alexis Georges; PONCELET, Virginie Sophie; ROUX, Bruno; MEERPOEL, Lieven; WO2013/61080; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of 2-Chloro-N-methylethanamine hydrochloride

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4535-90-4.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 4535-90-4

A mixture of 2-t-butylaniline (5.4 g) andmethylchlorethylamine hydrochloride (7 g) and K2C03 (5 g) inNal (2 g) in diglyme (150 m) was heated at 170 2C for 8 h.The reaction was filtered and the filtrate was evaporatedunder high vacuum. The residue was mixed with EtOAc (200 ml)and H20 (200 ml) and extracted with EtOAc twice. Thecombined organic layer was washed with brine and dried overNa2S04 and evaporated to give crude 1-[2-(tert-butylphenyl]-4-methylpiperazine. The crude 1-[2-(tert-butylphenyl]-4-methylpiperazine (260 mg) was stirred with H2S04 (3 ml) atOaC and HN03 (1.2 ml, 70%) was slowly added to the reaction.The reaction was warmed to RT, stirred for 30 min, poured onice and basified with K2C03 slowly. The solution wasextracted with EtOAc three times, washed with H20, followedby brine, dried over Na2S04 and evaporated under reducedpressure. The residue was purified by column chromatographyto give 1-[2-(tert-butyl)-5-nitrophenyl]-4-methylpiperazine(260 mg) , which was hydrogenated under H2 atmosphere to give1-[2-(tert-butyl)-5-aminophenyl]-4-methylpiperazine.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4535-90-4.

Reference:
Patent; AMGEN INC.; WO2006/12374; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 4535-90-4

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 4535-90-4, These common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

EXAMPLE 3 1,1a,6,10b-Tetrahydrodibenzo[a,e]cyclopropa[c]cyclohepten-6-one O-[ 2-(methylamino)ethyl]oxime SPC12 A dispersion of 1.5 g of 40% sodium hydride in mineral oil (0.025 mole of NaH) was thoroughly washed with hexane. To the sodium hydride, a solution of 2.4 g (0.010 mole) of 1,1a,6,10b-tetrahydrodibenzo[a,e]cyclopropa[c]cyclohepten-6-one oxime in 40 ml of dry hexamethylphosphoramide (HMPA) was added. The mixture was stirred at 25 for 1 hr under nitrogen. To the oxime salt was added 1.7 g (0.012 mole) of 2-methylaminoethylchloride hydrochloride and the mixture was stirred at 25 for 16 hrs. The reaction was processed as in Example 1 to give 2.5 g of an oil. Chromatography on 25 g of silica gel with ether as the eluent removed unreacted starting oxime. The crude product was obtained with methanol – 1% triethylamine as eluent. Flash distillation (0.1mu, 180 bath) of the methanol fractions gave 1,1a,6,10b-tetrahydrodibenzo[a,e]cyclopropa[c]cyclohepten-6-one O-[ 2-(methylamino)ethyl]oxime, MP 100- 101C. NMR spectrum (CDCL3): multiplet at delta6.8-7.5 (8H), triplet (J=6 Hz) at 4.2 (2H), triplet (J=6 Hz) at 2.8 (2H), singlet at 2.4 superimposed on a multiplet at 2.1-2.5 (5H) and a multiplet at 1.3-1.8 (3H). Mass. spec: Calcd. for C19 H20 N2 O: 292.1575; Found: 292.1546.

The synthetic route of 4535-90-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. Du Pont de Nemours & Company; US3960956; (1976); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Introduction of a new synthetic route about 4535-90-4

The synthetic route of 2-Chloro-N-methylethanamine hydrochloride has been constantly updated, and we look forward to future research findings.

Electric Literature of 4535-90-4, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 30 trans-(2-{8-Chloro-1-[4-(5-methyl-isoxazol-3-yl)-cyclohexyl]-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulen-5-yl}-ethyl)-methyl-amine A mixture of trans-8-chloro-1-[4-(5-methyl-isoxazol-3-yl)-cyclohexyl]-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene (50.0 mg, 0.130 mmol), cesium carbonate (170 mg, 0.521 mmol) and 2-methylaminoethyl chloride hydrochloride (67.7 mg, 0.521 mmol) in acetonitrile (1.3 ml) was heated at 70 C. for 20 h. After cooling to room temperature the reaction mixture was partitioned between 1 M aqueous sodium hydroxide solution (2 ml) and ethyl acetate (5 ml). The layers were separated. The aqueous layer was extracted with three 5-ml portions of ethyl acetate. The combined organic layers were concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid)/methanol as eluent gave the hydroformate salt of the title compound, which was liberated by filtration over aminopropyl modified silica gel (10 g) with methanol (20 ml) as eluent. The filtrate was concentrated to dryness. The residue was redissolved in ethyl acetate, filtrated over cotton wool and concentrated to dryness to give the title compound (38 mg, 66%) as off-white solid. MS m/e: 441 ([M+H]+).

The synthetic route of 2-Chloro-N-methylethanamine hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dolente, Cosimo; Schnider, Patrick; US2011/275801; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics